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JapanPositiveListSystem
TestMethodforSulfonylureaHerbicidesinAgriculturalProductsOasisHLB500mg/6cc,LC/MS
Iodosulfuron-methyl,Ethametsulfuron-methyl,Ethoxysulfuron,Cinosulfuron,Sulfosulfuron,Triasulfuron,Nicosulfuron,Pyrazosulfuron-ethyl,Primisulfuron-methyl,Prosulfuron&RimsulfuronTestMethod(Agriculturalproducts)
Analysiscompounds
Agro-chemicalsubstance
Analysiscompound
Iodosulfuron-methyl
Iodosulfuron-methyl&
Iodosulfuron-methylsodiumsalt
Ethametsulfuron-methyl
Ethametsulfuron-methyl
Ethoxysulfuron
Ethoxysulfuron
Cinosulfuron
Cinosulfuron
Sulfosulfuron
Sulfosulfuron
Triasulfuron
Triasulfuron
Nicosulfuron
Nicosulfuron
Pyrazosulfuron-ethyl
Pyrazosulfuron-ethyl
Primisulfuron-methyl
Primisulfuron-methyl
Prosulfuron
Prosulfuron
Rimsulfuron
Rimsulfuron
Apparatus
Liquidchromatograph,massspectrometer(LC/MS)
Reagents
UsethereagentslistedinSection2oftheGeneralRulesexceptforthefollowing:Acidicaluminaminicolumn(1710mg)
PEcolumntubeofinternaldiameter9-10mmfilledwithacidicalumina1710mgordevicethathasequivalentseparationcharacteristics.
(Sep-PakPlusLongAluminaA1710mg,P/NWAT020500)
Divinylbenzene-N-vinylpyrrolidoneco-polymerminicolumn(500mg)
PEcolumntubeofinternaldiameter12-13mmfilledwithDivinylbenzen-N-vinylpyrrolidoneco-polymer500mgordevicethathasequivalentseparationcharacteristics.
(OasisHLB500mg/6cc,P/N186000115)
StandardIodosulfuron-methyl Contains92%Iodosulfuron-methyl,meltingpoint152°CStandardEthametsulfuron-methylContains92%Ethametsulfuron-methyl,meltingpoint194°CStandardEthoxysulfuron Contains98%Ethoxysulfuronmeltingpoint144-147°CStandardCinosulfron Contains97%Cinosulfronmeltingpoint127-135°CStandardSulfosulfuron Contains97%Sulfosulfuronmeltingpoint201-202°CStandardTriasulfuron Contains98%Triasulfuronmeltingpoint178°C
StandardNicosulfuron Contains97%Nicosulfuronmeltingpoint169-172°CStandardPyrazosulfuron-ethyl Contains99%Pyrazosulfuron-ethylmeltingpoint178-180°CStandardPrimisulfuron-methyl Contains98%Primisulfuron-methylmeltingpoint195-197°CStandardProsulfuron Contains98%Prosulfuronmeltingpoint155°C
StandardRimsulfuron Contains99%Rimsulfuronmeltingpoint172-173°C
Procedure
Extraction
Forcereals,beansorseeds,take10.0goftestmaterial,add30mlofwaterandleavetostandfor2hours.Forfruits,vegetablesorherbs,use20.0g.
Addacetone100mL,andleavetostandfor60min(or30minforfruitsandvegetablesandherbs)afterhomogenization.Filterandcollectthefiltrate.Add50mLacetonetotheresidueonthefilter
paperandfilteragain.Combinethefiltratesandconcentrateto30mLunder40°Ccondition.
Add100mLof10%NaClsolutionand10mLof1mol/Lhydrogenchloride,thenextracttwicewith50mLethylacetate.Combinetheorganiclayers,addn-hexane100mL,andextracttwicewith50mL2%dipotassiumhydrogenphosphate.Add10gNaCland3mLof6mol/Lhydrogenchloride,andextracttwicein50mLethylacetate.Combinetheorganiclayersandaddanhydroussodiumsulfatetodry.Filtertoremovetheanhydroussodiumsulfate.Evaporatethefiltrateunder40°Ccondition.Dissolvetheresidueinacetone,andmakeuptoexactly10mL(or20mLforfruitsandvegetablesandherbs).
Clean-up
Acidicaluminacolumnchromatography
Addacetonitrile10mLandacetone10mLtoconditiontheacidicaluminacolumn(1710mg)(Sep-PakPlusLongAluminaA1710mg,P/NWAT020500).Discardtheeffluent.Afterloading2mLofsamplesolutionfromextractionstep1)intothecolumn,discardtheeffluent.Then,washwith8mLacetoneand20mLacetonitrile,anddiscardtheeffluent.Next,elutewith10mLacetonitrile/water(9:1).Evaporateeluantunder40°Ccondition.Dissolvetheresiduewith10mLwater.
Divinylbenzene-N-vinylpyrrolidoneco-polymercolumnchromatography
Conditionthedivinylbenzene-N-vinylpyrrolidoneco-polymerminicolumn(500mg)(OasisHLB500mg/6cc,P/N186000115)with10mLmethanoland10mLwater,anddiscardtheeffluent.Afterloadingthesampleobtainedinclean-upstep1)tothecolumn,discardtheeffluent.Then,washwith
10mLwater/methanol(4:1),anddiscardtheeffluent.Next,elutewith15mLmethanol,andevaporatetheeluantunder40°Ccondition.Dissolvetheresiduein1mLacetonitrile/water(1:1).
Calibrationcurves
Diluteeachstandard,Iodosulfuron-methyl,Ethametsulfuron-methyl,Ethoxysulfuron,Cinosulfuron,Sulfosulfuron,Triasulfuron,Nicosulfuron,Pyrazosulfuron-ethyl,Primisulfuron-methyl,Prosulfuron&Rimsulfuronwithacetonitrile/water(1:1)solutiontomakeseveralconcentrationsofmixedstandardsolutionswithin0.02-0.4mg/L.Inject4μLeachintoLC/MS.Usepeaksintheresultingchromatogramstopreparecalibrationcurvesusingthepeakheightorpeakareamethod.
Determination
Inject4μLoftestsolutionintoLC/MSanddeterminethecontentsofIodosulfuron-methyl,Ethametsulfuron-methyl,Ethoxysulfuron,Cinosulfuron,Sulfosulfuron,Triasulfuron,Nicosulfuron,Pyrazosulfuron-ethyl,Primisulfuron-methyl,Prosulfuron&RimsulfuronusingLC/MSorLC/MS/MSresultsandthecalibrationcurvespreparedintheabovestep5.ForIodosulfuron-methyl,multiplytheIodosulfuron-methyl-sodiumsaltanalysisresultby0.96.
Confirmation
PerformLC/MSmeasurement.
Measuringconditions
LC/MS
ForEthametsulfuron-methyl,Ethoxysulfuron,Cinosulfuron,Sulfosulfuron,Triasulfuron,Nicosulfuron,Pyrazosulfuron-ethyl,Primisulfuron-methyl&Rimsulfuron:
Column:Octadecylsilanizedsilicagel(particlediameter5μm,internaldiameter2-3mm,length150mm)
Columntemperature:40°C
Mobilephase:Gradientfrom1%formicacidtoacetonitrile/1%formicacidmixture(19:1)over20minutes.
IonizedMode:ESI(+)Majorion(m/z):
Ethametsulfuron-methyl&Nicosulfuron 411
Ethoxysulfuron
399
Cinosulfuron
414
Sulfosulfuron
471
Triasulfuron
402
Pyrazosulfuron-ethyl
415
Primisulfuron-methyl
469
Rimsulfuron
432
Expectedretentiontime:Primisulfuron-methyl20min
ForIodosulfuron-methylandProsulfuron:
Column:Octadecylsilanizedsilicagel(particlediameter5μm,I.D.2-3mm,length150mm)Columntemperature:40°C
Movingphase:Gradientfrom1%formicacidtoacetonitrile/1%formicacidmixture(19:1)over20minutes.
IonizedMode:ESI(-)
Majormonitoringion(m/z):
Iodosulfuron-methyl
506
Prosulfuron
418
Expectedretentiontime:Prosulfuron19.5min
9.Limitofquantitation
0.01mg/kg
Others
Testmethodoutline
Iodosulfuron-methyl,Ethametsulfuron-methyl,Ethoxysulfuron,Cinosulfuron,Sulfosulfuron,Triasulfuron,Nicosulfuron,Pyrazosulfuron-ethyl,Primisulfuron-methyl,Prosulfuron&Rimsulfuronareextractedfromtestmaterialusingacetone,andconvertedintoethylacetateinacidicstate,andreverse-extractedusingdipotassiumhydrogenphosphate.Thiswillbeconvertedagainintoethylacetateunderacidicstate.Afterclean-upwithacidicaluminamini-columnanddivinylbenzene-N-vin
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